EP4206190A1 - Raffinierungsverfahren für acesulfam - Google Patents

Raffinierungsverfahren für acesulfam Download PDF

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Publication number
EP4206190A1
EP4206190A1 EP20953772.9A EP20953772A EP4206190A1 EP 4206190 A1 EP4206190 A1 EP 4206190A1 EP 20953772 A EP20953772 A EP 20953772A EP 4206190 A1 EP4206190 A1 EP 4206190A1
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Prior art keywords
ace
crystal
solution
preset
crystals
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English (en)
French (fr)
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EP4206190A4 (de
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Congchun WANG
Yongxu CHEN
Xiaofeng Shen
Chaohui Chen
Dongdong Shen
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Anhui Jinhe Industrial Co Ltd
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Anhui Jinhe Industrial Co Ltd
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Publication of EP4206190A1 publication Critical patent/EP4206190A1/de
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
    • C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
    • C07D291/06—Six-membered rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00—Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13—Crystalline forms, e.g. polymorphs

Definitions

  • the present disclosure belongs to the field of fine chemical manufacturing, and in particular relates to a method for refining acesulfame potassium (Ace K).
  • a refining process includes: separating an organic phase to obtain a mother liquor, commonly known as syrup; subjecting the mother liquor to a series of steps such as decolorization, heating concentration, freezing crystallization, and centrifugal separation to obtain raw sugar ( Yu Jiang, Synthesis Research of Sweetener Acesulfame-K, "Science and Technology Innovation Herald” 2008, 35, 9 ); and subjecting the raw sugar to recrystallization at least twice to obtain a qualified Ace K product.
  • the biggest difficulty during the production and refining of Ace K is that organic impurities produced in the production may be carried from an initial sugar to a final product, resulting in excessive organic impurities in the sugar and a relatively dark color of the product.
  • the purification process from syrup to qualified products is intermittent, which has high energy consumption and serious waste of resources for multiple crystallization, cumbersome human operations, and high production costs, as well as complex and diverse reaction device, large temperature changes, and short service life of the equipment.
  • intermittent production due to intermittent production, the utilization rate of the device is low, and the impurity content of the finished product is likely to exceed the standards. Accordingly, the product has a quality that cannot meet market requirements, seriously affecting its market value.
  • a method for refining Ace K is provided in the present disclosure to overcome the above problems or at least partially solve the above problems.
  • a method for refining Ace K including the following steps:
  • an Ace K crystal prepared by the method for refining Ace K, where the Ace K crystal has a purity of greater than 99.20%, an organic impurity content of lower than 10 ppm, and a moisture content of lower than 0.3 wt%.
  • Some embodiments provide by the present disclosure have the following beneficial effects: by controlling the pretreatment, a solution to be crystallized (i.e., the syrup) is subjected to oxidative decolorization, which reduces the content of organic impurities in the initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product.
  • oxidative decolorization reduces the content of organic impurities in the initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product.
  • oxidative decolorization which reduces the content of organic impurities in the initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product.
  • crystallization process and technology a high-quality and high-purity crystallization product is obtained with a less impurity content, and
  • FIG. 1 shows an X-ray diffraction (XRD) pattern of Ace K crystals prepared according to Example 1 and Comparative Example 1.
  • an concept lies in that: a solution to be crystallized (i.e. syrup) of Ace K is oxidized and decolorized through oxidation-reduction and physical adsorption, so as to reduce the content of organic impurities in the initial sugar; the initial sugar forms a crystal nucleus through concentration and heat preservation; and the crystal nucleus is fully crystallized through secondary nucleation, such that an Ace K crystal is obtained with a desirable crystal form and a high purity, thereby significantly reducing the impurity content of peritectic and improving a purity of the product.
  • a method for refining Ace K includes the steps as described below: Pretreatment: adding hydrogen peroxide and activated carbon to an Ace K crude product-containing solution to obtain a mixture, maintaining the mixture at a first preset temperature for a first preset time, and filtering the mixture to obtain an Ace K mother liquor.
  • the Ace K crude product solution obtained in the Ace K production contains a large number of organic impurities, such as acetoacetamide, and further contains some colored impurities, such as compounds produced by dimerization of diketene, including diacetyl trisphenol and trimerized tetrafenpyrrole ( E. Marcus and J. K. Chan, Novel Confensation Products of Diketene, J. Org. Chem. 1967, 32, 9, 2881-2887 .).
  • impurities such as acetoacetamide and multimers are treated with hydrogen peroxide.
  • the hydrogen peroxide reacts with acetoacetamide and multimers in the organic impurities to undergo oxidation-reduction to generate hydrophilic carboxylic acids and the like.
  • substances such as hydrophilic carboxylic acids remain in the solution and do not enter the final product.
  • activated carbon a type of specially-treated carbon.
  • Heating organic raw materials such as husks, coal, and wood
  • a carbonization product reacts with the gas such that the surface of the carbonization product is eroded to produce a microporous structure, which is called activation.
  • Activation is a microscopic process, that is, the surface erosion of a large number of molecular carbides is point erosion, resulting in countless fine pores on the surface of activated carbon.
  • the surface micropores of activated carbon have diameters of mostly 2 nm to 50 nm.
  • Nucleation conducting concentration on the Ace K mother liquor to a preset concentration to obtain a concentrated solution, allowing the concentrated solution to stand at a second preset temperature for a second preset time to form an Ace K crystal nucleus, and obtaining a crystal nucleus-containing solution.
  • Crystallization conducting programmed freezing on the crystal nucleus-containing solution to obtain a solution with a large number of Ace K crystals.
  • a process for forming crystals includes two steps, one corresponding to the nucleation and the other corresponding to the crystallization.
  • the nucleation is to form a small amount of crystal nuclei in the Ace K mother liquor by controlling conditions; these nuclei act as seed crystal during the crystallization, providing a basis for the massive growth of crystals.
  • Ace K crystals are generally obtained through repeated recrystallization. There are many defects in the crystals generated in this way, such as low purity of the product, low yield, complex process, and high requirements for equipment and personnel skills.
  • the existing crystallization is divided into two steps, where the formation of crystal nuclei of Ace K is promoted through the control of conditions; and based on the formed crystal nuclei, the rapid formation of a large number of Ace K crystals is promoted by means of programmed freezing.
  • a high-purity and high-yield Ace K crystal product can be obtained through conventional post-treatment techniques, including but not limited to centrifugation, water washing, and drying.
  • a solution to be crystallized i.e., the syrup
  • oxidative decolorization which reduces a content of organic impurities in the initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product.
  • oxidative decolorization reduces a content of organic impurities in the initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product.
  • a high-quality and high-purity crystallization product is obtained with a less impurity content, and purity and quality of the Ace K crystal are significantly improved.
  • the method for refining Ace K has a simple process, mild and controllable conditions, and low requirements for equipment and personnel skills, which is extremely suitable for large-scale industrial production.
  • the hydrogen peroxide is present in an amount of 0.1 wt% to 10 wt%, preferably 0.5 wt% to 2 wt% of a total mass of the Ace K crude product-containing solution. Since the amount of organic impurities in the Ace K crude product-containing solution is predictable or estimable, the dosage of hydrogen peroxide can be determined according to a total mass of the Ace K crude product-containing solution. If the amount of hydrogen peroxide is less than 0.1 wt% of the total mass of the Ace K crude product-containing solution, hydrogen peroxide has an insufficient amount, and thus cannot completely neutralize the reducing organic impurities.
  • the amount of hydrogen peroxide is more than 10 wt% of the total mass of the Ace K crude product-containing solution, hydrogen peroxide has an excessive amount, and the excess hydrogen peroxide may corrode equipment due to strong oxidizing properties, making the post-treatment complicated and difficult to handle.
  • the amount of the activated carbon is in an amount of 0.1 wt% to 5 wt%, preferably 0.2 wt% to 4 wt% of a total mass of the Ace K crude product-containing solution. Since the amount of colored impurities in the Ace K crude product-containing solution is predictable or estimable, the dosage of activated carbon can be determined according to a total mass of the Ace K crude product-containing solution. If the amount of activated carbon is less than 0.1 wt% of the total mass of the Ace K crude product-containing solution, the activated carbon has an insufficient amount, and thus cannot completely absorb the colored impurities in the Ace K crude product-containing solution. If the amount of activated carbon is more than 5 wt% of the total mass of the Ace K crude product-containing solution, the amount is excessive, causing unnecessary waste, and increasing the burden on subsequent filtering procedures.
  • the pretreatment two reactions occur simultaneously: redox chemical reaction between hydrogen peroxide and organic impurities, and the physical adsorption of activated carbon on colored impurities.
  • the two reactions can only achieve a desired effect under certain conditions.
  • the first preset temperature is in the range of 40°C to 90°C; and the first preset time is in the range of 1 h to 8 h.
  • the redox chemical reaction and physical adsorption cannot be completed due to too mild conditions and too short contact time. If the first preset temperature is greater than 90°C and the first preset time is greater than 8 h, the redox chemical reaction and physical adsorption are too sharp due to too intense conditions and too long contact time; especially, the redox chemical reaction may even cause localized bumping.
  • the concentration is conducted by vacuum distillation at a temperature of 45°C to 80°C, preferably 55°C to 65°C and at a pressure of -95 KPa to -101 KPa for 10 min to 12 min.
  • the conditions for the vacuum distillation are to quickly make the Ace K mother liquor reach the preset concentration without causing excessive load to the equipment.
  • the preset concentration is that a solid phase accounts for 30 wt% to 90 wt%, preferably 40 wt% to 80 wt% of a total mass of the Ace K mother liquor.
  • the preset concentration may be related to whether subsequent crystal nuclei and crystals can be successfully generated.
  • concentration if the content of the solid phase in the Ace K mother liquor is less than 30 wt% of a total mass of the Ace K mother liquor, there may be too much solvent, making it difficult to generate crystal nuclei in the subsequent nucleation. If the content of the solid phase in the Ace K mother liquor is greater than 90 wt% of the total mass of the Ace K mother liquor, there may be too little solvent, resulting in rapid evaporation of the solvent during the subsequent heat preservation of the nucleation, and the formed crystal nuclei and crystals cannot be effectively separated. As a result, a large number of irregular crystals are generated, which may even lead to failure of the entire refining.
  • the second preset temperature is in the range of 40°C to 70°C, preferably 45°C to 60°C; and the second preset time is in the range of 0.1 h to 4 h, preferably 0.5 h to 2 h.
  • the temperature and time for heat preservation may be important parameters to promote the nucleation. If these parameters are not properly controlled, crystal nuclei cannot be generated.
  • the second preset temperature is in the range of 40°C to 70°C, and the second preset time is in the range of 0.1 h to 4 h; and in some other embodiments, the preset temperature is in the range of 45°C to 60°C, and the second preset time is in the range of 0.5 h to 2 h. If the second preset temperature is less than 40°C, the temperature is too low, which may cause the solvent to evaporate too slowly during the nucleation, making it difficult to precipitate crystal nuclei.
  • the second preset temperature is greater than 60°C, the temperature is too high, which may result in extremely irregular crystal nuclei being precipitated during the nucleation.
  • the time also requires a lot of investigation. If the second preset time is shorter than 0.1 h, the time is too short, which may cause the crystal nuclei to not yet precipitate or the crystal nuclei to just start to precipitate or only a small amount of crystal nuclei to precipitate; too few crystal nuclei cannot provide an effective seed crystal for subsequent crystallization. If the second preset time is longer than 2 h, the time is too long, which may cause a large amount of crystal nuclei precipitated; even some crystals with complicated crystal forms are produced, which are not the crystal forms expected in the present disclosure.
  • the programmed freezing conditions may be a key directly related to whether a large amount of high-quality crystals can be formed quickly; in some embodiments, the programmed freezing includes: cooling down from the second preset temperature to an intermediate temperature of 40°C to 45°C at a rate of 1°C/10 min to 1°C/60 min and holding the intermediate temperature for 0.5 h to 8 h, and then cooling down from the intermediate temperature to 8°C to 12°C at a rate of 1°C/10 min to 1°C/60 min.
  • the programmed freezing includes: cooling down from the second preset temperature to an intermediate temperature of 45°C at a rate of 1°C/10 min to 1°C/60 min and holding the intermediate temperature for 0.5 h to 8 h, and cooling down from the intermediate temperature to 10°C at a rate of 1°C/10 min to 1°C/60 min.
  • a high-purity Ace K crystal can be obtained by any one of the above methods.
  • the Ace K crystal has a purity of higher than 99.30%, an organic impurity content of lower than 10 ppm, and a moisture content of lower than 0.3 wt%.
  • Ace K in an existing Ace K product generally has a purity of 93.0 wt% to 99.0 wt%, and it is difficult to achieve a purity of more than 99.0%.
  • the Ace K product prepared by the refining method provided in the present disclosure has a purity of greater than 99.0%, an organic impurity content of lower than 10 ppm, and a moisture content of lower than 0.3 wt%.
  • the Ace K crystals prepared according to some embodiments in the present disclosure are measured by XRD. Before drying, the Ace K crystal has three strongest diffraction peaks at 8.8 ⁇ 0.2, 17.3 ⁇ 0.2, and 28.8 ⁇ 0.2, respectively; and after drying, the Ace K crystal has an XRD spectrum peak intensity weaker than that of the Ace K crystal before drying, showing a strongest diffraction peak at 8.8 ⁇ 0.2 and a second strongest diffraction peak at 17.3 ⁇ 0.2. It can be seen that the prepared wet Ace K sample has a desirable crystal structure, showing simple and strong XRD peaks; after the sample is dried to obtain an anhydrous sample, a part of the crystal structure is destroyed, and the XRD peaks of the sample are also weaker than those before drying.
  • test methods adopted in each example and comparative example are as follows, and are not repeated in each example.
  • the methods for analysis and test of Ace K could refer to the national standard of food additives GB/T5009.140-2003, "Determination of acesulfame K (Ace K) in beverages”.
  • Ace K high-performance liquid chromatograph of Shimadzu, Japan (ultraviolet detector), LC-10ADVP high-pressure pump, CTO-10ASVP constant-temperature box; chromatographic column: Agilent XDB C18 column (250 mm ⁇ 4.6 mm, 5 ⁇ m); mobile phase: 0.02 mol/L ammonium sulfate (780 mL) + methanol (100 mL) + acetonitrile (30 mL); column temperature: 30°C; and flow rate: 0.8 mL/min. The content was measured by an external standard method.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 20 wt % of Ace K
  • the mixture was stirred and subjected to heat preservation at 80°C for 2 h, and then the activated carbon was then removed by filtration while the mixture was hot.
  • a resulting syrup solution was concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h to a preset concentration of 30 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 60°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 45°C at 1°C/20 min and subjected to heat preservation at the intermediate temperature for 2 h, and then cooled to about 10°C at 1°C/20 min to obtain a large number of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 25 g of a high-purity solid crystal with a purity of 99.5%, an impurity content of 10 ppm, and a moisture content of 0.2 wt%.
  • FIG. 1 shows an XRD pattern of the samples measured before and after drying.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 20 wt % of Ace K
  • a to-be-crystallized Ace K solution obtained in a previous process was directly concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h until a solid concentration of the Ace K was 30 wt% to obtain an Ace K mother liquor, and the Ace K mother liquor was rapidly cooled to 10°C, and crystallized for 12 h to obtain a large amount of crystals.
  • Fig. 1 shows an XRD pattern of the samples measured before and after drying.
  • Example 1 and Comparative Example 1 show that 25 g of an Ace K solid was prepared according to Example 1, and 21 g of an Ace K solid was prepared according to Comparative Example 1, indicating that the yield of Ace K crystals of Example 1 is far greater than that of Comparative Example 1.
  • Fig. 1 shows the XRD pattern of Ace K crystals prepared according to Example 1 and Comparative Example 1.
  • Curves 1 and 3 show the XRD pattern of the Ace K samples prepared according to Example 1 and Comparative Example 1 before drying, respectively, i.e. the XRD pattern of the wet samples; and curves 2 and 4 show the XRD pattern of the Ace K samples prepared according to Example 1 and Comparative Example 1 after drying, respectively, i.e. the XRD pattern of the dry samples.
  • the crystals obtained by the two methods according to Example 1 and Comparative Example 1 have extremely large differences in structure:
  • a to-be-crystallized Ace K solution i.e., syrup, containing 20 wt % of Ace K
  • the mixture was stirred and subjected to heat preservation at 80°C for 2 h, and the activated carbon was then removed by filtration while the mixture was hot.
  • a resulting syrup solution was concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h to a preset concentration of 40 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 60°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 45°C at 1°C/10 min and subjected to heat preservation at the intermediate temperature for 1 h, and then cooled to about 10°C at 1°C/10 min to obtain a large number of crystals.
  • a resulting solution containing the crystal was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 31 g of a high-purity solid crystal a purity of 99.2%, an impurity content of 20 ppm, and a moisture content of 0.3 wt%.
  • Fig. 1 shows an XRD pattern of the samples measured before and after drying.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 20 wt % of Ace K
  • the mixture was stirred and subjected to heat preservation at 80°C for 2 h, and the activated carbon was then removed by filtration while the mixture was hot.
  • a resulting syrup solution was concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h to a preset concentration of 45 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 50°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 40°C at 1°C/30 min and subjected to heat preservation at the intermediate temperature for 2 h, and then cooled to about 10°C at 1°C/30 min to obtain a large number of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 32g of a high-purity solid crystal a purity of 99.6%, an impurity content of 4 ppm, and a moisture content of 0.2 wt%.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 25 wt % of Ace K
  • the mixture was stirred and subjected to heat preservation at 70°C for 2 h, and the activated carbon was then removed by filtration while the mixture was hot.
  • a resulting syrup solution was concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h to a preset concentration of 45 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 50°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 40°C at 1°C/30 min and subjected to heat preservation at the intermediate temperature for 2 h, and then cooled to about 10°C at 1°C/30 min to obtain a large number of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 40g of a high-purity solid crystal a purity of 99.5%, an impurity content of 6 ppm, and a moisture content of 0.2 wt%.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 25 wt % of Ace K
  • the mixture was stirred and subjected to heat preservation at 80°C for 2 h, and the activated carbon was then removed by filtration while the mixture was hot.
  • a resulting syrup solution was concentrated by vacuum distillation at -0.095 MPa and 70°C for 1 h to a preset concentration of 45 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 50°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 40°C at 1°C/30 min and subjected to heat preservation at the intermediate temperature for 2 h, and then cooled to about 10°C at 1°C/30 min to obtain a large number of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 42 g of a high-purity solid crystal a purity of 99.2%, an impurity content of 15 ppm, and a moisture content of 0.2 wt%.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 25 wt % of Ace K
  • a to-be-crystallized Ace K solution obtained in a previous process was heated and distilled, 0.5 g of activated carbon was added, stirred and subjected to heat preservation at 70°C for 2 h, and the activated carbon was removed by filtration while the mixture was hot.
  • the treated resulting syrup solution was concentrated by vacuum distillation (-0.095 MPa, 70°C) for 1 h to a preset concentration of 40 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 55°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 45°C at 1°C/10 min and subjected to heat preservation for 1 h at the intermediate temperature, and then cooled to about 10°C at 1°C/10 min to obtain a large amount of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 38 g of a high-purity solid crystal a purity of 99.2%, an impurity content of 35 ppm, and a moisture content of 0.3 wt%.
  • a to-be-crystallized Ace K solution i.e., syrup, containing 25 wt % of Ace K
  • a to-be-crystallized Ace K solution obtained in a previous process was heated and distilled, 0.5 g of hydrogen peroxide was added, stirred and subjected to heat preservation at 80°C for 2 h, and concentrated by vacuum distillation (-0.095 MPa, 70°C) for 1 h to a preset concentration of 40 wt%.
  • a resulting concentrated solution was subjected to heat preservation at 60°C for 1 h to form an effective crystal nucleus.
  • a resulting crystal nucleus-containing solution was cooled to an intermediate temperature of about 45°C at 1°C/10 min and subjected to heat preservation for 1 h at the intermediate temperature, and then cooled to about 10°C at 1°C/10 min to obtain a large amount of crystals.
  • a resulting solution containing the crystals was centrifuged and washed with a small amount of cold ultrapure water to obtain a wet centrifuged sample, and then dried to obtain 37 g of a high-purity solid crystal a purity of 99.2%, an impurity content of 25 ppm, and a moisture content of 0.3 wt%.
  • Comparative Example 2 and Comparative Example 3 the to-be-crystallized Ace K solution was pretreated by a single substance. As shown in the results of Example 5 and Comparative Examples 2-3, the final products according to Comparative Examples 2-3 have a higher impurity content than that of the final product obtained by using both hydrogen peroxide and activated carbon to simultaneously pretreat the to-be-crystallized Ace K solution.
  • Example 2 and Comparative Examples 2-3 From Example 2 and Comparative Examples 2-3, it can be seen that the yield of Ace K crystals in Example 2 is significantly higher than that of Comparative Examples 2-3, indicating that the yield of the final product obtained by pretreatment of the to-be-crystallized Ace K solution with both hydrogen peroxide and activated carbon is higher than that of the final product obtained by pretreatment of the to-be-crystallized Ace K solution by a single substance.
  • the refining effects of Example 1 and Comparative Example 1 are obviously not as good as that of Examples 2 to 5.
  • a solution to be crystallized i.e., the syrup
  • oxidative decolorization which reduces a content of organic impurities in initial sugar of Ace K and prevents the organic impurities from being brought into a final crystallization product, resulting in defects such as low purity and yellow color of the product
  • crystallization process and technology a high-quality and high-purity crystallization product is obtained with a less impurity content, and purity and quality of the Ace K crystal are significantly improved; moreover, the method for refining Ace K has a simple process, mild and controllable conditions, and low requirements for equipment and personnel skills, which is extremely suitable for large-scale industrial production.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Saccharide Compounds (AREA)
EP20953772.9A 2020-09-21 2020-09-21 Raffinierungsverfahren für acesulfam Pending EP4206190A4 (de)

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